CNT STABILITY WITHIN POLYMER NANOCOMPOSITE MEMBRANE MATRICES

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1 CNT STABILITY WITHIN POLYMER NANOCOMPOSITE MEMBRANE MATRICES Nov. 3 rd, 2013 Charles-François de Lannoy, Katie Gloe, and Prof. Mark Wiesner

2 Sustainable Material Development and Use Exposure Concern NP Losses Material production Material incompatibility NP Leaching Long term material instability Lifetime exposures and interactions Uncertain Environmental Fates Develop Chemically Compatible Materials Test Expected Uses and Exposures

3 Case Study: Membranes and CNTs (Sulfonated) Polysulfone (PSf) Ultrafiltration Membranes Hand Cast Flat sheet Immersion Precipitated Dissolved in NMP or DMF Functionalized Multiwalled Carbon Nanotubes CVD grown d = 8 15 nm L = µm Functionalized with amines or carboxylic acids

4 Novel Technologies for Water Supply and Treatment Water Supply Water Re-Use Water Filtration Desalination Water Treatment Wastewater Treatment Industrial Water Treatment

5 Most Important Membrane Parameters Selectivity Flux Control Over the Type of Molecule that Passes Through Microfiltration (MF), Ultrafiltration (UF), Nanofiltration (NF) Reverse Osmosis (RO), Forward Osmosis (FO), Membrane Distillation (MD) Control Over How Quickly Water Passes Through High Water Flux Low Pressures, FO, MD

6 Predominant Membrane Shortcomings Membrane surface Bacterial biofilm 20 µm 200 µm Breakages Vibrational Stresses Break Membranes Fouling Biofouling Organic Matter Fouling Scaling High Energy Costs Passive Treatment Membranes don t degrade contaminants

7 Multiwalled Carbon Nanotubes (MWCNTs) High Tensile Strength ~1 Tpa, 1000x stronger than steel Entirely sp 2 hybridized carbon Large van der Waals Forces Highly hydrophobic and bundle Difficult to disperse in most solvents 500 nm

8 Covalent Carboxylation of CNTs 13/ nm 20 nm Break π-bonds in sp 2 hybridized carbon atoms Create defects along their length Greatly improve homogeneous dispersion Change surface chemistry Carboxyl, COO Hydroxyl, OH Amine, NH + 2

9 Many Possible CNT-Polymer Interactions CNT Functionalizations Used Covalent Functionalization Polymer Chain Cross-linking Monomer Polymerization Ionic Bonding Charge Association Non-Covalent Functionalization Polymer Wrapping Non-Covalent Covalent

10 Stability of Bulk Mixed fcnts in Polymers Vary Degree of Functionalization CNT-COOHs in PSf Varying Percent functionalization Investigate Stability Measure Membrane Properties Test how CNT-COOHs affect Membrane

11 Counts Per Second Binding Energy (ev) XPS Evidence of CNT Carboxylation C 1s C-C, C=C CNT backbone C=O C=O C-O C O

12 Bulk Mixed Polymer Composites PSf-PVP-CNT Solution Sonicate CNTs in solvent to disperse Blend with PVP to wrap Dissolve PSf with PVPwrapped CNTs Hand cast membrane Phase inversion in nonsolvent to gel

13 Responsible Use of Nanomaterials PSf-CNT CNTs in bulk polymer matrices Active Side is darker High and low functionalization produces lighter color Color correlates to CNT dispersion and content

14 CNTs Lost During Membrane Fabrication Loss of CNTs from membranes during precipitation immersion is measured by UV-Vis absorption PSf-CNT

15 CNTs Leached During Membrane Cleaning Leaching from membranes due to cleaning agents is measured by UV-Vis absorption PSf-CNT

16 Effect of fcnts and CNT Loss on Young s Modulus

17 Effect of fcnts and Loss on Surface Chemistry θ

18 Sulfonated Polysulfone 18/22 CH 3 O (CH 3 ) 3 SiO 3 Cl CH 3 O C O S CH 3 Bisphenol-A Polysulfone, PSf (Udel-P1700) O O trimethylsilyl chlorosulfonate C O S CH 3 O SO 3 Si(CH 3 ) 3 O HCl MeONa CH 3 O MeOH C O S CH 3 O O (CH 3 ) 3 SiOCH 3 SO 3 - Na + Sulfonated Bisphenol-A Polysulfone (PSSNa) CH 3 O C O S O CH 3 O SO 3 - Na + - HO + H 3 N - HO + H 3 N NH 3 + NH 3 + OH - NH 3 + NH 3 + OH - (10,0) Zigzag

19 Ionic Bonding Prevents CNT Loss

20 Effect on Young s Modulus

21 Effect on Surface Chemistry

22 Complications to the Story Membrane Morphology Changes Ionic bonding changes polymer orientation and precipitation Alters Surface Porosity Alters Internal Membrane Structure Negative Repercussions on Membrane Properties

23 Conclusions Non-covalently bound CNTs leach from membranes Greater CNT functionalization leads to greater loss Loss of CNTs during membrane precipitation Leaching of CNTs during membrane cleaning Loss of CNTs has negative repercussions on membrane properties Ionic bonding between polymer and CNTs eliminates loss of CNTs Leaching prevention rectifies property trends Ionic bonding has negative repercussions on other membrane propertes

24 Acknowledgements Prof. Mark Wiesner, CEINT, Duke University Prof. Elif Soyer, Marmara University Katie Gloe, Virginia Tech

25 Many Possible CNT Functionalizations Covalent Functionalizations Most Common CNT Functionalizations Carboxyl, COO Hydroxyl, OH Amine, NH 2 +

26 Polymer Theory 26/24 Flory-Huggins Theory Hildebrand Solubility Parameters

27 PSf-PVP-CNT MF/UF Membrane Fabrication Bundled unfunctionalized CNTs 2 µm Dispersed carboxylated CNTs 500 nm 2 µm

28 Functionalizing CNTs for Polymer Compatibility Carboxylic Acid Functionalization Bulk wet chemistry approach Sulfuric:Nitric acid reflux Centrifuge and/or filter dialyse to raise ph Acid groups added Predominantly (-COOH) Lesser degree (-OH)

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